Аннотация:The synthesis of a phosphinic structural analogue of the tetrapeptide Met-Glu-γ-His-Phe by adding the dipeptide component His-Phe to the adamantyl ester of the phosphinic pseudo-Met-[P]-Glu-peptide in the form of cyclic glutamate anhydride is proposed. The conditions for the interaction of phosphinic pseudo-Met-[P]-Gluanhydride with His-Phe in free form to form phosphinic Met-[P]-Glu-γ-His-Phe tetrapeptide have been found. A chromatographic mass-spectrometry study, including MS2, and NMR of the phosphinic tetrapeptide on 1H, 13C, 31P nuclei was carried out using the methods of two-dimensional 1H–1H COSY, 1H–13C HSQC and 1H–13C HMBC NMR spectroscopy.